CN104404289A - High-pore controllable three-dimensional through hole foam molybdenum and preparation method thereof - Google Patents
High-pore controllable three-dimensional through hole foam molybdenum and preparation method thereof Download PDFInfo
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- CN104404289A CN104404289A CN201410764918.3A CN201410764918A CN104404289A CN 104404289 A CN104404289 A CN 104404289A CN 201410764918 A CN201410764918 A CN 201410764918A CN 104404289 A CN104404289 A CN 104404289A
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Abstract
The invention discloses a high-pore controllable three-dimensional through hole foam molybdenum and a preparation method thereof. The molybdenum pore is in the shape of a three-dimensional sphere, and the pore is formed by mutually communicating generating holes with interstitial holes. The pore rate of the molybdenum structure is higher and is controllable, the pore is in the shape of a regular sphere, and the pore has isotropic mechanical characteristic. The preparation method is based on a traditional powder metallurgy method, a foaming method is combined, a novel layer spread method for material loading is adopted, and then, the foam molybdenum is obtained through pressing, dissolving and sintering. The preparation method provided by the invention is simple, the cost is low, the production cycle is short, pores are distributed uniformly, and the foam molybdenum has favorable mechanical and energy absorption properties.
Description
Technical field
The present invention relates to a kind of porous metal material, particularly a kind of have high porosity controlled three-dimensional through-hole foam molybdenum of high hole being evenly communicated with three-dimensional pore texture and preparation method thereof.
Background technology
Porous metal material combines conduction, heat conduction, can weld and the metallic character such as plastic and hypertonicity, energy absorption, capillarity, back-fire relief and the distinctive functional performance of vesicular structure such as heat insulation, is industrially widely used in the High Speed Fields such as filtration & separation, damping, fire prevention, permeator and aerospace.Comprehensive literature is reported, the research major part of porous metal material concentrates on light metal and low melting material, and this constrains porous material application under extreme conditions greatly.The fusing point of molybdenum is up to 2620 DEG C, and less than 1000 DEG C have good resistance to corrosion, do not inhale hydrogen, is suitable for high temperature occasion and some other special occasions.Porous molybdenum or with porous molybdenum for the various components and parts that matrix makes are widely used in the fields such as modern light technology, pyrotic smelting, electronic vacuum, heat control system, energy industry, nuclear technique and medical science.It will become very important function and structured material in high-new and extreme field gradually.
Porous Mo all needs through-hole structure to a great extent being applied in of field such as infiltration, filtration, heat exchange, catalytic carrier, liquid stream adjustable attenuation, biomedical material and shape memory devices.The porosity of through-hole foamed metal material and pore size are very important structural parameter, as just needed comparatively accurate porosity and pore size in strainer and fluid control.In addition, large quantity research shows, the porosity of porous material and the mechanical property tool of pore size to material have a great impact, and the specific rigidity performance tool of such as porosity to material has a significant impact shock resistance simultaneously and compression performance also has very large contact with porosity and pore size.
Although through development and the research of decades, the preparation of porous material makes great progress, but the foam metal material that existing Technology obtains or performance index are inadequate, or cost is too high, especially the preparation cost of through-hole foamed metal is higher, and porosity and connectedness are also difficult to control simultaneously.According to the difference of hole incorporation way, the preparation technology of through-hole foamed metal material mainly contains: 1, compacting sintering method, by metal-powder directly compression moulding in a mold, sinters subsequently.2, organic matrix soaking paste drying and sintering method, is mixed with slurry by powder, and by the leaching of the organic matrix of porous with wherein, the porous organic matrix after soaking paste process carries out drying and sintering.3, foaming, mixes whipping agent with metal-powder and suppresses, and is removed by whipping agent subsequently and carries out powder sintered.Foaming is a kind of simple to operate, preparation method with low cost, the thinking that it prepares porous material is mixed among powder by whipping agent, then adopts heating or dissolution method to be removed by whipping agent according to the character feature of whipping agent, form the hole substantially identical with size with whipping agent position.What foaming was formed is the pore texture that the mesopore that between creating holes and powder, hole is formed stayed after whipping agent is removed is interconnected and surrounds.A critical process of foaming is the batch mixing process of whipping agent and metal-powder, method for mixing general at present adopts mixer to carry out batch mixing, but when whipping agent differs larger with metal-powder particle diameter, the phenomenon of whipping agent segregation will be inevitably there is in batch mixing process, have a strong impact on homogeneity and the connectedness of hole, and then affect material property.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides that a kind of porosity is high and controlled, even pore distribution and controlled three-dimensional through-hole foam molybdenum of the high hole be interconnected and preparation method thereof.The preparation method of material provided by the present invention is simple, and cost is low, even pore distribution, has good mechanics and energy absorption.
The technical scheme that the present invention solves the problems of the technologies described above is:
The controlled three-dimensional through-hole foam molybdenum of a kind of high porosity, this molybdenum hole is three-dimensional spherical, and hole is interconnected by creating holes and mesopore and forms.
The preparation method of the controlled three-dimensional through-hole foam molybdenum of above-mentioned high porosity, comprises the steps such as charging, compacting, dissolving, sintering, selects spherical urea to be pore-forming material, uses " layer spread method " to obtain evenly and the pore texture be communicated with, specifically comprises the steps:
(1) by porosity requirement, convert and the quality of molybdenum powder needed for taking out every layer and urea;
(2) molybdenum powder taken is loaded in mould, then wire cloth is put into mould, pour the urea weighed up into, pull-out wire netting makes urea be uniformly distributed in molybdenum powder, urea is gently pressed to make it embed in molybdenum powder with depression bar, urea is distributed in molybdenum powder matrix equably, obtains equally distributed pore texture;
(3) above-mentioned two steps repeated 4-6 time, namely layer paving is 6-9mm to powder mix height;
(4) carry out dissolving after layer paving, dry, sintering, the controlled three-dimensional through-hole foam molybdenum of high porosity can be obtained.
The preparation method of the controlled three-dimensional through-hole foam molybdenum of above-mentioned high porosity, the conversion relation of described every layer of molybdenum powder quality and required porosity is: M
mo=R*S* (1-P) * ρ
mo, the conversion relation of every layer of urea quality and required porosity is: M
c=S*R*P* ρ
c, M
m0for the quality of molybdenum powder, M
cfor the quality of urea, R is the diameter of urea, and S is mould cross-sectional area, and P is porosity, ρ
mofor molybdenum powder density, ρ
cfor urea density.
The controlled three-dimensional through-hole foam molybdenum of above-mentioned high porosity, R=1.2mm, S=153.9mm
2, ρ
mo=10.21g/cm
3, ρ
c=1.335g/cm
3, p=75%, 70% or 65%.
The preparation method of the controlled three-dimensional through-hole foam molybdenum of above-mentioned high porosity, described molybdenum powder particle diameter is 74 μm, and described urea diameter is 1mm.
The preparation method of the controlled three-dimensional through-hole foam molybdenum of above-mentioned high porosity, described compression moulding adopts hydropress, and pressure is 300Mpa; Described dissolving adopts hot water, and hot water temperature is 60 DEG C, and dissolution time is 2 hours; Described drying temperature is 250 DEG C, and the time is 3 hours; Describedly be sintered to vacuum sintering, temperature is 1800 DEG C, and the time is 3 hours.
Three-dimensional pore texture molybdenum of the present invention, by selecting the spherical urea of regular shape to be foam material, in conjunction with novel loading method, obtains the three-dimensional through-hole porous body of high porosity.The feature of porous insert is: the creating holes that hole is formed after dissolving primarily of urea and the mesopore composition that inter-granular porosity is formed, mesopore is interconnected as the minim channel between creating holes and creating holes and surrounds, porosity communication, porosity and pore dimension are determined by the addition of urea and size.
Beneficial effect of the present invention is:
(1) molybdenum pore texture of the present invention be rule solid spherical, there is good isotropy.
(2) molybdenum porosity of the present invention is high, and is evenly distributed, and is interconnected between hole.
(3) molybdenum structure of the present invention, its hole is interconnected primarily of the micropore of equally distributed spherical macropore and stochastic distribution and forms, and both ensure that the isotropy of mechanical property in turn ensure that the connectedness of hole.
(4) preparation method of the present invention is simple, easy to operate, with low cost, practical.
Accompanying drawing explanation
Fig. 1 is layer spread method charging process schematic diagram of the present invention.
Fig. 2 is the macro morphology figure that the embodiment of the present invention 1 to 3 and comparative example prepare molybdenum, shows that molybdenum structure porosity obtained by embodiment 1 to 3 is high, even pore distribution, spherical void pattern rule in figure; And the standby porosity of comparative example common batch mixing legal system is the porous molybdenum macro morphology figure of 70%, shows its hole generation segregation, skewness.
Fig. 3 is that the three-dimensional that the present invention prepares molybdenum surpasses depth of field microstructure photograph, shows the effect that is interconnected in this structure between spherical creating holes.
Fig. 4 is the low power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 to 3 prepares molybdenum, shows in this structure and there is the micropore that yardstick is several microns in figure, and widely distributed, becomes the passage between creating holes.
Fig. 5 is the particle combined that the embodiment of the present invention 1 to 3 prepares molybdenum, and showing above-mentioned micropore in figure is be combined into by intergranular crane span structure, also show the intergranular sintering of molybdenum in porous insert and bonding state simultaneously.
Fig. 6 is the parameter of pore structure of embodiment 1 to 3 different porosities sample, and these parameters show that pore dimension keeps urea size used substantially, and pore texture is controlled.
Fig. 7 is the dynamic compressing stress strain curve figure that the embodiment of the present invention 1 to 3 prepares molybdenum, the figure illustrates the present invention prepare the mechanical property of molybdenum and shock resistance good.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further details, but the present invention is not limited to this.
Embodiment 1
Preparation porosity is the molybdenum of 75%
Step 1) weighing.Calculating quality needed for every layer of molybdenum powder by required porosity and every layer of molybdenum powder, urea quality relation formula is 0.392g, and quality needed for urea is 0.154g.The molybdenum powder of 74 μm is divided into 0.392g every part, and urea is divided into 0.154g every part.
Step 2) charging.The 1 part of molybdenum powder weighed up in step 1 is loaded mould, molybdenum powder is flattened with depression bar, put into wire cloth, then 1 part of urea is imported mould, mould is put into by wire cloth, pour the urea weighed up into, pull-out wire netting also gently presses urea with depression bar, makes urea granules occur to reset and embeds equably between molybdenum powder (idiographic flow is see Fig. 1).Repeat above-mentioned charging process 5 times.
Step 3) compacting.By feeding in step 2, complete mould is pressed into base in 300MPa on a hydraulic press.
Step 4) dissolve.Gained green compact in step 3 are put into 60 DEG C of hot water and soak 3h to remove the urea of green compact.
Step 5) dry and sintering.In step 4, after gained dissolving, green compact put into resistance furnace with 250 DEG C of dryings 3 hours, load in vacuum sintering furnace subsequently, 10
-3with the ramp to 1800 DEG C of 6 DEG C/min under the vacuum environment of Pa, insulation 3h, insulation terminates rear furnace cooling.
Embodiment 2
Preparation: preparation porosity is the molybdenum of 70%
Calculating quality needed for every layer of molybdenum powder by required porosity and every layer of molybdenum powder, urea quality relation formula is 0.471g, and quality needed for urea is 0.143g.The molybdenum powder of 74 μm is divided into 0.471g every part, and urea is divided into 0.143g every part.All the other steps are with embodiment 1.
Embodiment 3
Preparation: preparation porosity is the molybdenum of 65%
Calculating quality needed for every layer of molybdenum powder by required porosity and every layer of molybdenum powder, urea quality relation formula is 0.55g, and quality needed for urea is 0.133g.The molybdenum powder of 74 μm is divided into 0.55g every part, and urea is divided into 0.133g every part.All the other steps are with embodiment 1.
Comparative example
Common batch mixing legal system is for the molybdenum of porosity 70%
The ratio being 8:3 in mass ratio by molybdenum powder and urea mixes in mixer, and all the other compactings are dissolved and the complete same above-described embodiments of sintering step, and finally obtain the vesicular structure of void distribution inequality, its macroscopic form is shown in Fig. 2.
Claims (9)
1. the controlled three-dimensional through-hole foam molybdenum of high porosity, is characterized in that: this molybdenum hole is for three-dimensional spherical, and hole is interconnected by creating holes and mesopore and forms.
2. the preparation method of the controlled three-dimensional through-hole foam molybdenum of high porosity according to claim 1, is characterized in that comprising the steps:
(1) by porosity requirement, convert and the quality of molybdenum powder needed for taking out every layer and urea;
(2) loaded in mould by the molybdenum powder taken, then wire cloth is put into mould, pour the urea weighed up into, pull-out wire netting makes urea be uniformly distributed in molybdenum powder, gently presses urea to make it embed in molybdenum powder with depression bar;
(3) above-mentioned two steps repeated 4-6 time, namely layer paving is 6-9mm to powder mix height;
(4) carry out dissolving after layer paving, dry, sintering, the controlled three-dimensional through-hole foam molybdenum of high porosity can be obtained.
3. the preparation method of the controlled three-dimensional through-hole foam molybdenum of high porosity according to claim 2, is characterized in that: the conversion relation of described every layer of molybdenum powder quality and required porosity is: M
mo=R*S* (1-P) * ρ
mo, the conversion relation of every layer of urea quality and required porosity is: M
c=S*R*P* ρ
c, M
m0for the quality of molybdenum powder, M
cfor the quality of urea, R is the diameter of urea, and S is mould cross-sectional area, and P is porosity, ρ
mofor molybdenum powder density, ρ
cfor urea density.
4. the preparation method of the controlled three-dimensional through-hole foam molybdenum of high porosity according to claim 3, is characterized in that: R=1.2mm, S=153.9mm
2, ρ
mo=10.21g/cm
3, ρ
c=1.335g/cm
3, p=75%, 70% or 65%.
5. the preparation method of the controlled three-dimensional through-hole foam molybdenum of the high porosity according to any one of claim 2 to 4, it is characterized in that: described molybdenum powder particle diameter is 74 μm, described urea diameter is 1mm.
6. the preparation method of the controlled three-dimensional through-hole foam molybdenum of the high porosity according to any one of claim 2 to 4, is characterized in that: described compression moulding adopts hydropress, and pressure is 300Mpa.
7. the preparation method of the controlled three-dimensional through-hole foam molybdenum of the high porosity according to any one of claim 2 to 4, is characterized in that: described dissolving adopts hot water, and hot water temperature is 60 DEG C, and dissolution time is 2 hours.
8. the preparation method of the controlled three-dimensional through-hole foam molybdenum of the high porosity according to any one of claim 2 to 4, it is characterized in that: described drying temperature is 250 DEG C, the time is 3 hours.
9. the preparation method of the controlled three-dimensional through-hole foam molybdenum of the high porosity according to any one of claim 2 to 4, is characterized in that: described in be sintered to vacuum sintering, temperature is 1800 DEG C, and the time is 3 hours.
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| CN107010902A (en) * | 2017-05-12 | 2017-08-04 | 湘潭大学 | A kind of macroporous structure soil and its method for making sample |
| CN107486559A (en) * | 2017-09-01 | 2017-12-19 | 中南大学 | A kind of aluminium base density gradient material and its preparation method and application |
| CN107876775A (en) * | 2017-10-27 | 2018-04-06 | 兰州理工大学 | A kind of porous Ti of structure-controllable low damage processing method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105543513A (en) * | 2015-12-19 | 2016-05-04 | 湖南科技大学 | Molybdenum-copper composite material in three-dimensional communicated reticular structure and preparation method of molybdenum-copper composite material |
| CN107010902A (en) * | 2017-05-12 | 2017-08-04 | 湘潭大学 | A kind of macroporous structure soil and its method for making sample |
| CN107486559A (en) * | 2017-09-01 | 2017-12-19 | 中南大学 | A kind of aluminium base density gradient material and its preparation method and application |
| CN107486559B (en) * | 2017-09-01 | 2019-09-24 | 中南大学 | A kind of aluminium base density gradient material and its preparation method and application |
| CN107876775A (en) * | 2017-10-27 | 2018-04-06 | 兰州理工大学 | A kind of porous Ti of structure-controllable low damage processing method |
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